Method for continuously preparing 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene in gas phase

A technology of trifluoromethyl and fluoromethyl is applied in the field of gas-phase continuous preparation of 3,3,3-trifluoro-2--1-propene, which can solve the problem of low yield, low product yield and easy clogging of pipelines and other problems, to achieve the effect of long service life and high activity

Active Publication Date: 2021-07-09
泉州宇极新材料科技有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

There are following problems in this route: the temperature of second step reaction is too high, can produce a large amount of waste solid metal fluorides, and the productive rate of product is lower
This route has the following disadvantages: (1) raw materials are difficult to obtain; (2) a large amount of waste ammonium salts will be produced
This route has the following problems: (1) the liquid phase process is adopted, and a large amount of solvent is used, which will generate a large amount of waste liquid and waste solid, which seriously pollutes the environment; (2) raw materials are difficult to obtain
This route has the following problems: (1) raw materials are difficult to obtain; (2) the second step reaction uses a large amount of KOH as a dehydrochlorination reagent, which will produce a large amount of waste solids, and the intermediate 3-chloro-3,3-difluoro-2- The yield of trifluoromethyl-1 propene is too low, resulting in too low single-pass yield of the whole route for the synthesis of 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene
This route has the following problems: (1) the total yield is too low; (2) the gas phase continuous method has certain industrial value, but the effective metering of sulfur is a technical challenge, and it is easy to block the pipeline, so the pipeline and measuring instruments Insulation is important
This route has the following problems: (1) raw materials are difficult to obtain, and the yield is low; (2) SF 4 is a highly toxic substance
This route has the following defects: (1) The second and fourth steps use a large amount of solvent and a large amount of solid strong base, which will produce a large amount of liquid waste and solid waste, which seriously pollutes the environment; (2) The first and third steps The hydrogenation reaction is a batch process, and the yield of the product is low
[0024] So far, there is no 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene in the open literature that satisfies the characteristics of easy availability of raw materials, high yield per pass, and easy realization of continuous gas phase production. synthetic route

Method used

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  • Method for continuously preparing 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene in gas phase
  • Method for continuously preparing 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene in gas phase
  • Method for continuously preparing 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene in gas phase

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preparation example Construction

[0061] 1. Preparation of hydrogenation catalyst:

[0062] (1) Preparation of the carrier of the hydrogenation catalyst: Dissolve aluminum trichloride in water, add concentrated ammonia water dropwise for precipitation, adjust the pH value to 7.5, then age for 24 hours, wash with water, filter, and dry in an oven at 120°C for 15 hour, the gained solid is pulverized, pressed into tablets, and the precursor of the carrier is obtained, and the precursor 10mL of the carrier is packed into a tubular reactor with an internal diameter of 1 / 2 inch and a length of 30cm. ℃ roasting for 12 hours, nitrogen space velocity is 200h -1 , and then lower the temperature to 300°C, and at the same time pass a mixed gas composed of hydrogen fluoride and nitrogen with a mass ratio of 1:2, and the total space velocity of the gas is 220h -1 , activated for 12 hours, stop the above gas mixture, and produce aluminum fluoride.

[0063] Other supports can be prepared by substituting other soluble metal ...

Embodiment 1

[0070] 2%Pd / 98%AlF is filled in a tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30cm 3 Catalyst 10mL. The reaction conditions are as follows: the reaction temperature is 50°C, the mass ratio of octafluoroisobutene to hydrogen is 1:10, the contact time is 60s, and the reaction pressure is 0.1MPa. After running for 10 hours, the reaction product was washed with water, washed with alkali and dried, and the gas phase organic phase was taken for GC analysis. The reaction results are: the conversion rate of octafluoroisobutene is 73.4%, and the selectivity of 1,1,1,3,3,3-hexafluoro-2-(difluoromethyl)propane is 99.8%.

Embodiment 2

[0072] 2%Pd / 98%AlF is filled in a tubular reactor made of Incon alloy with an inner diameter of 1 / 2 inch and a length of 30cm 3 Catalyst 10mL. The reaction conditions are as follows: the reaction temperature is 100°C, the mass ratio of octafluoroisobutene to hydrogen is 1:10, the contact time is 60s, and the reaction pressure is 0.1MPa. After running for 10 hours, the reaction product was washed with water, washed with alkali and dried, and the gas phase organic phase was taken for GC analysis. The reaction results are: the conversion rate of octafluoroisobutene is 93.8%, and the selectivity of 1,1,1,3,3,3-hexafluoro-2-(difluoromethyl)propane is 99.6%.

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Abstract

The invention discloses a method for continuously preparing 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene in gas phase, which uses octafluoroisobutene as a raw material through hydrogenation-dehydrofluorination-hydrogenation-dehydrogenation Four-step gas-phase continuous reaction of hydrogen fluoride to obtain 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene. Both the hydrogenation catalyst and the dehydrofluorination catalyst of the present invention have the characteristics of high activity and long service life; and through the gas phase independent circulation process, the incompletely reacted materials can be independently circulated, so that the initial raw materials can be almost completely converted3,3, 3‑trifluoro‑2‑(trifluoromethyl)‑1‑propene, and finally the product 3,3,3‑trifluoro‑2‑(trifluoromethyl) is extracted from the process system with high efficiency and continuous gas phase circulation )‑1‑propylene, so that no liquid waste and waste gas are produced, and green production is realized.

Description

technical field [0001] The invention relates to a method for continuously preparing 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene in a gas phase, in particular to a method for taking octafluoroisobutene as a starting material, which is subjected to gas phase hydrogenation, gas phase A method for synthesizing 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene by four steps of dehydrofluorination, gas-phase hydrogenation, and gas-phase dehydrofluorination. Background technique [0002] At present, the existing synthetic routes of 3,3,3-trifluoro-2-(trifluoromethyl)-1-propene mainly include the following seven kinds: [0003] Route 1: Starting from hexafluoropropylene and difluoromethane [0004] [0005] The literature "Journal of Fluorine Chemistry 108 (2001) 15-20" and patent EP1175380 reported the synthesis of 3,3,3-trifluoro- The technical route of 2-(trifluoromethyl)-1-propene: (1) The first step reaction: under the action of antimony pentafluoride, react hexafluoropropen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/25C07C21/18C07C17/354C07C19/08
CPCC07C17/25C07C17/354C07C21/18C07C19/08
Inventor 张呈平贾晓卿董利权恒道
Owner 泉州宇极新材料科技有限公司
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